The suitability of purge-trap-desorb (PTD) procedures for determination of 84 volatile organic compounds with capillary column gas chromatograph (GC) and mass spectrometry (MS) was evaluated. After collecting GC-MS data not previously available for some analytes, 7 of the 84 compounds were eliminated from further consideration because of poor purging efficiency or analyte instability. For each of the remaining 77 compounds, the linear concentration range and detection limit were determined with data obtained by PTD GC-MS analysis of spiked reagent water. The criterion was met over a concentration range of at least two orders of magnitude for 56 of the 77 analytes, 1.5 orders of magnitude for 12 analytes, and 1 order of magnitude for 6 analytes. The criterion was not met for acetone, trichlorofluoromethane, and 2-chloro-1,3-butadiene. Method performance was assessed by analyzing eight replicate aliquots of two simulated liquid waste samples (a municipal sewage sludge leachate and water containing fulvic acid) containing analytes spiked at two concentrations.